CN105219083A - Fire retardant utilizing organo-silicone rubber waste material to produce and preparation method thereof - Google Patents
Fire retardant utilizing organo-silicone rubber waste material to produce and preparation method thereof Download PDFInfo
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Abstract
The invention discloses a kind of fire retardant utilizing organo-silicone rubber waste material to produce and preparation method thereof, organo-silicone rubber waste material 18-35 part, trimeric cyanamide 5-10 part, phenyl trichlorine silicon gastral cavity 5-10, silane coupling agent 1-6 part, highly basic 5-16 part, alcohol 80-110 part, deionized water 20-50 part, fire-resistant synergistic composition 4-19 part.Hydrophobic performance of the present invention is fine, and polyacrylic flame retardant properties can be made to significantly improve, does flame retardant properties reach UL-94? V-0 level, limiting oxygen index(LOI) can reach more than 38.5%.In addition, the situation of being fuming when polypropylene also can be made to burn and drippage situation, and the mechanical property of material (tensile strength, flexural strength and shock strength) also be improved significantly.
Description
Technical field
The present invention relates to the recycling field of organo-silicone rubber waste material, specifically a kind of fire retardant utilizing organo-silicone rubber waste material to produce and preparation method thereof.
Background technology
Organo-silicone rubber is owing to having outstanding resistance to elevated temperatures, oxidation-resistance, ageing resistance, weathering resistance and cryogenic subduing flexibility, and its range of application is more and more extensive.But, its expensive raw material price, and always have waste material to occur in machine-shaping and application.These waste materials are due to through high temperature vulcanized, and molecular chain is cross-linked with each other, therefore can not natural degradation; If do not dealt carefully with, can serious environment pollution.At present, how to reclaim waste material and by its Appropriate application once again, attract the sight of people with the Sustainable development realizing resource.
Current macromolecular material superpolymer has been widely used in industrial production and daily life.Most of macromolecular material superpolymer is all inflammable, in flammable solid fire, occupy dominant position.Therefore the macromolecular material superpolymer of flame retardant type becomes a primary study direction of Material Field, and additive flame retardant is the most widely used at present.At present, additive flame retardant year usage quantity more than 1,000,000 tons.Wherein: (1) does not produce toxic gas and corrosive gases although inorganic combustion inhibitor is as fire-retardant in magnesium hydroxide and aluminium hydroxide have simultaneously with when pressing down cigarette effect and burn, and has a strong impact on by the physics of fire retardant material, mechanical property and processing characteristics because required addition is comparatively large.(2) although organic halogenated flame retardant has the features such as high flame retardant efficiency and high performance-price ratio, because its HX playing fire retardation is poisonous corrosive gases, be harmful to environment and human body, therefore its Application Areas has been restricted, and oneself is eliminated gradually.(3) halogen-free flame retardants (IFR) has low cigarette, the advantage such as nontoxic, and IFR for essential core composition, can produce cooperative flame retardant effect with phosphorus, nitrogen, carbon when being heated; Composite IFR usually with ammonium polyphosphate (APP) for acid source, with trimeric cyanamide (MEL) for whipping agent, with tetramethylolmethane (PER) for char-forming agent, by the carbonaceous foam layer that can generate even compact during high heat, can heat insulation, oxygen barrier, press down cigarette, anti-molten drop, there is good flame retardant properties; But this based flame retardant mostly is hydrophilic, with polymer base poor compatibility, and required addition is comparatively large, have impact on the physicals of flame retarded polymeric material superpolymer, therefore can not meet the demand of macromolecular material.(4) organic silicon fibre retardant is that the one of development in recent years is new and effective, low toxicity, anti-molten drop, eco-friendly halogen-free flame retardants, is also a kind of charcoal becoming smoke suppressant.Organic silicon fibre retardant, outside the flame retardant properties of giving base material excellence, can also improve the processing characteristics of base material, resistance toheat etc.; But because price is more expensive, application is also subject to a definite limitation.
According to Britain's " polymer degradation is with stable " (PolymerDegradationandStability, 90:523-534,2005) introduce, add the polypropylene flame redardant obtained by the expanding fire retardant be made up of trimeric cyanamide ammonium sulfate and tetramethylolmethane accounting for system total mass 40% and just can reach UL-94V0 rank, but the mechanical property of material such as tensile strength and breaking tenacity can be caused to decline because the total amount of adding expanding fire retardant is comparatively large.
According to the U.S.'s " polymer science magazine " (JournalofPolymerScience, partA:Ploymerchemistry42:6163-6173,2004) introduce, during by organo montmorillonite and expansion type flame retardant synergistic polypropylene flame redardant, when to account for system total mass percentage composition ratio be 4% to organo montmorillonite quality, the heat release rate of polypropylene flame redardant obviously can be reduced; But along with the increase (after more than 4%) of organo montmorillonite content aggravates because reuniting, its flame retardant effect declines on the contrary.
In addition, although existing employing melt-blending process obtains have the characteristics such as LSZH and resistance to molten containing nitrogen-phosphorus expansion fire retardant or the flame-retardant polymer containing nitrogen-phosphorus expansion fire retardant and retardant synergist, but flame retardant effect is still not ideal enough, resistance to molten property need to improve, also because the flame retardant amount of required interpolation can make comparatively greatly the mechanical property of material such as tensile strength, breaking tenacity decline, and production cost is higher.
Summary of the invention
The object of the present invention is to provide a kind of cheapness, environmental protection, good flame retardation effect and fire retardant utilizing organo-silicone rubber waste material to produce not affecting macromolecular material superpolymer mechanical property and preparation method thereof.
For achieving the above object, the invention provides following technical scheme:
Utilize the fire retardant that organo-silicone rubber waste material is produced, according to the raw material of weight part be: organo-silicone rubber waste material 18-35 part, trimeric cyanamide 5-10 part, phenyl trichlorine silicon gastral cavity 5-10, silane coupling agent 1-6 part, highly basic 5-16 part, alcohol 80-110 part, deionized water 20-50 part, fire-resistant synergistic composition 4-19 part;
Described fire-resistant synergistic composition according to the component of weight part is: carbon nanotube 4-6 part, nano mesoporous molecular screen 4-6 part, nano-attapulgite 4-6 part, micron silicon nitride 1-3 part, micrometer silicon carbide silicon 1-3 part.
Further, described fire-resistant synergistic composition according to the component of weight part is: carbon nanotube 4 parts, nano mesoporous molecular screen 5 parts, nano-attapulgite 5 part, micron silicon nitride 2 parts, micrometer silicon carbide silicon 2 parts.
Further, described silane coupling agent be in KH550 silane coupling agent, KH560 silane coupling agent and KH570 silane coupling agent any one or multiple.
Further, described highly basic is sodium hydroxide and/or potassium hydroxide.
Further, the carbonatoms of described alcohol is 2-6.
Further, described nano mesoporous molecular screen be in MCM-41 mesopore molecular sieve, MCM-48 mesopore molecular sieve, SBA-15 mesopore molecular sieve and SBA-16 mesopore molecular sieve any one or multiple.
The preparation method of the fire retardant utilizing organo-silicone rubber waste material to produce, is characterized in that, concrete steps are:
(1) first organo-silicone rubber waste powder is broken into the particle that particle diameter is not more than 2mm, then adds reactor with silane coupling agent, highly basic together with unit alcohol, under stirring, microwave heating, to 30-90 DEG C, is incubated 1-3 hour; The power of described microwave heating is 0.8-1.2kW, and frequency is 1200-3600MHz;
(2) add deionized water extraction after filtering, standing separation, takes off layer liquid and is placed in reactor;
(3) in reactor, trimeric cyanamide, phenyl trichlorine silicon gastral cavity and fire-resistant synergistic composition is added again, under stirring, supersound process 0.5-1.5 hour; The power of described ultrasonication is 150-250W, and frequency is 20-40kHz;
(4) cool, filter, washing reaction product, after drying, namely obtains the fire retardant utilizing organo-silicone rubber waste material to produce.
Further, in step (1), microwave heating is to 40-60 DEG C, insulation 1.5-2.5 hour; The power of described microwave heating is 0.9-1.1kW, and frequency is 2000-2800MHz.
Further, supersound process 0.8-1.2 hour in step (3); The power of described ultrasonication is 180-220W, and frequency is 25-35kHz.
Compared with prior art, the invention has the beneficial effects as follows:
The fire retardant hydrophobic performance that the present invention utilizes organo-silicone rubber waste material to produce is fine, and add in polypropylene, polyacrylic flame retardant properties can be made to significantly improve, and flame retardant properties reaches UL-94V-0 level, and limiting oxygen index(LOI) can reach more than 38.5%.In addition, the situation of being fuming when polypropylene also can be made to burn and drippage situation, and the mechanical property of material (tensile strength, flexural strength and shock strength) also be improved significantly.
Embodiment
Be described in more detail below in conjunction with the technical scheme of embodiment to this patent.
Embodiment 1
Utilize the fire retardant that organo-silicone rubber waste material is produced, according to the raw material of weight part be: 22 parts, organo-silicone rubber waste material, trimeric cyanamide 8 parts, phenyl trichlorine silicon gastral cavity 6 parts, KH550 silane coupling agent 2 parts, 5 parts, sodium hydroxide, ethanol 80 parts, deionized water 30 parts, fire-resistant synergistic composition 2 parts; Described fire-resistant synergistic composition according to the component of weight part is: carbon nanotube 6 parts, MCM-41 mesopore molecular sieve 4 parts, nano-attapulgite 4 part, micron silicon nitride 1 part, micrometer silicon carbide silicon 1 part.
The preparation method of the described fire retardant utilizing organo-silicone rubber waste material to produce, concrete steps are:
(1) first organo-silicone rubber waste powder is broken into the particle that particle diameter is not more than 2mm, then adds reactor with silane coupling agent, highly basic together with unit alcohol, under stirring, microwave heating, to 30 DEG C, is incubated 3 hours; The power of described microwave heating is 0.8kW, and frequency is 1200MHz;
(2) add deionized water extraction after filtering, standing separation, takes off layer liquid and is placed in reactor;
(3) in reactor, trimeric cyanamide, phenyl trichlorine silicon gastral cavity and fire-resistant synergistic composition is added again, under stirring, supersound process 1.5 hours; The power of described ultrasonication is 150W, and frequency is 20kHz;
(4) cool, filter, washing reaction product, after drying, namely obtains the fire retardant utilizing organo-silicone rubber waste material to produce.
The present embodiment product yield is 92.3%; 300 DEG C of calcinations 30 minutes in retort furnace, weightless 1.5%, product is placed and within water one week, does not sink, illustrate that hydrophobic performance is fine.
Embodiment 2
Utilize the fire retardant that organo-silicone rubber waste material is produced, according to the raw material of weight part be: 30 parts, organo-silicone rubber waste material, trimeric cyanamide 10 parts, phenyl trichlorine silicon gastral cavity 5 parts, KH560 silane coupling agent 4 parts, 12 parts, potassium hydroxide, tetramethylolmethane 100 parts, deionized water 40 parts, fire-resistant synergistic composition 11 parts; Described fire-resistant synergistic composition according to the component of weight part is: carbon nanotube 5 parts, MCM-48 mesopore molecular sieve 5 parts, nano-attapulgite 5 part, micron silicon nitride 2 parts, micrometer silicon carbide silicon 2 parts.
The preparation method of the described fire retardant utilizing organo-silicone rubber waste material to produce, concrete steps are:
(1) first organo-silicone rubber waste powder is broken into the particle that particle diameter is not more than 2mm, then adds reactor with silane coupling agent, highly basic together with unit alcohol, under stirring, microwave heating, to 60 DEG C, is incubated 2 hours; The power of described microwave heating is 1kW, and frequency is 2400MHz;
(2) add deionized water extraction after filtering, standing separation, takes off layer liquid and is placed in reactor;
(3) in reactor, trimeric cyanamide, phenyl trichlorine silicon gastral cavity and fire-resistant synergistic composition is added again, under stirring, supersound process 1 hour; The power of described ultrasonication is 200W, and frequency is 30kHz;
(4) cool, filter, washing reaction product, after drying, namely obtains the fire retardant utilizing organo-silicone rubber waste material to produce.
The present embodiment product yield is 93.4%; 300 DEG C of calcinations 30 minutes in retort furnace, weightless 1.2%, product is placed and within water one week, does not sink, illustrate that hydrophobic performance is fine.
Embodiment 3
Utilize the fire retardant that organo-silicone rubber waste material is produced, according to the raw material of weight part be: 35 parts, organo-silicone rubber waste material, trimeric cyanamide 9 parts, phenyl trichlorine silicon gastral cavity 8 parts, KH570 silane coupling agent 6 parts, 15 parts, highly basic, ethanol 120 parts, deionized water 50 parts, fire-resistant synergistic composition 20 parts; Described fire-resistant synergistic composition according to the component of weight part is: carbon nanotube 6 parts, SBA-16 mesopore molecular sieve 6 parts, nano-attapulgite 6 part, micron silicon nitride 3 parts, micrometer silicon carbide silicon 3 parts.
The preparation method of the described fire retardant utilizing organo-silicone rubber waste material to produce, concrete steps are:
(1) first organo-silicone rubber waste powder is broken into the particle that particle diameter is not more than 2mm, then adds reactor with silane coupling agent, highly basic together with unit alcohol, under stirring, microwave heating, to 90 DEG C, is incubated 1 hour; The power of described microwave heating is 1.2kW, and frequency is 3600MHz;
(2) add deionized water extraction after filtering, standing separation, takes off layer liquid and is placed in reactor;
(3) in reactor, trimeric cyanamide, phenyl trichlorine silicon gastral cavity and fire-resistant synergistic composition is added again, under stirring, supersound process 1.5 hours; The power of described ultrasonication is 250W, and frequency is 40kHz;
(4) cool, filter, washing reaction product, after drying, namely obtains the fire retardant utilizing organo-silicone rubber waste material to produce.
The present embodiment product yield is 92.5%; 300 DEG C of calcinations 30 minutes in retort furnace, weightless 1.3%, product is placed and within water one week, does not sink, illustrate that hydrophobic performance is fine.
Comparative example 1
Utilize the fire retardant that organo-silicone rubber waste material is produced, according to the raw material of weight part be: 30 parts, organo-silicone rubber waste material, trimeric cyanamide 10 parts, phenyl trichlorine silicon gastral cavity 5 parts, KH560 silane coupling agent 3 parts, 10 parts, potassium hydroxide, tetramethylolmethane 100 parts, deionized water 40 parts.
The preparation method of the described fire retardant utilizing organo-silicone rubber waste material to produce, concrete steps are:
(1) first organo-silicone rubber waste powder is broken into the particle that particle diameter is not more than 2mm, then adds reactor with silane coupling agent, highly basic together with unit alcohol, under stirring, microwave heating, to 60 DEG C, is incubated 2 hours; The power of described microwave heating is 1kW, and frequency is 2400MHz;
(2) add deionized water extraction after filtering, standing separation, takes off layer liquid and is placed in reactor;
(3) in reactor, trimeric cyanamide is added again, under stirring, supersound process 1 hour; The power of described ultrasonication is 200W, and frequency is 30kHz;
(4) cool, filter, washing reaction product, after drying, namely obtains the fire retardant utilizing organo-silicone rubber waste material to produce.
The present embodiment product yield is 86.7%; 300 DEG C of calcinations 30 minutes in retort furnace, weightless 4.5%, product is placed and within water one week, does not sink, illustrate that hydrophobic performance is fine.
Comparative example 2
Utilize the fire retardant that organo-silicone rubber waste material is produced, according to the raw material of weight part be: 30 parts, organo-silicone rubber waste material, trimeric cyanamide 8 parts, phenyl trichlorine silicon gastral cavity 9 parts, KH560 silane coupling agent 3 parts, 10 parts, potassium hydroxide, tetramethylolmethane 100 parts, deionized water 40 parts, fire-resistant synergistic composition 11 parts; Described fire-resistant synergistic composition according to the component of weight part is: carbon nanotube 5 parts, MCM-48 mesopore molecular sieve 5 parts, nano-attapulgite 5 parts.The preparation method of the described fire retardant utilizing organo-silicone rubber waste material to produce, with embodiment 2.
The present embodiment product yield is 89.8%; 300 DEG C of calcinations 30 minutes in retort furnace, weightless 2.4%, product is placed and within water one week, does not sink, illustrate that hydrophobic performance is fine.
Comparative example 3
Utilize the fire retardant that organo-silicone rubber waste material is produced, according to the raw material of weight part be: 30 parts, organo-silicone rubber waste material, trimeric cyanamide 10 parts, KH560 silane coupling agent 3 parts, 10 parts, potassium hydroxide, tetramethylolmethane 100 parts, deionized water 40 parts, fire-resistant synergistic composition 11 parts; Described fire-resistant synergistic composition according to the component of weight part is: micron silicon nitride 3 parts, micrometer silicon carbide silicon 3 parts.The preparation method of the described fire retardant utilizing organo-silicone rubber waste material to produce, with embodiment 2.
The present embodiment product yield is 90.1%; 300 DEG C of calcinations 30 minutes in retort furnace, weightless 2.2%, product is placed and within water one week, does not sink, illustrate that hydrophobic performance is fine.
Comparative example 4
Utilize the fire retardant that organo-silicone rubber waste material is produced, according to the raw material of weight part be: 30 parts, organo-silicone rubber waste material, trimeric cyanamide 6 parts, phenyl trichlorine silicon gastral cavity 8 parts, KH560 silane coupling agent 3 parts, 10 parts, potassium hydroxide, tetramethylolmethane 100 parts, deionized water 40 parts, fire-resistant synergistic composition 11 parts; Described fire-resistant synergistic composition according to the component of weight part is: carbon nanotube 5 parts, MCM-48 mesopore molecular sieve 5 parts, nano-attapulgite 5 part, micron silicon nitride 2 parts, micrometer silicon carbide silicon 2 parts.
The preparation method of the described fire retardant utilizing organo-silicone rubber waste material to produce, concrete steps are:
(1) first organo-silicone rubber waste powder is broken into the particle that particle diameter is not more than 2mm, then adds reactor with silane coupling agent, highly basic together with unit alcohol, under stirring, be electrically heated to 60 DEG C, be incubated 2 hours;
(2) add deionized water extraction after filtering, standing separation, takes off layer liquid and is placed in reactor;
(3) in reactor, add trimeric cyanamide and fire-resistant synergistic composition again, stir 2 hours;
(4) cool, filter, washing reaction product, after drying, namely obtains the fire retardant utilizing organo-silicone rubber waste material to produce.
The present embodiment product yield is 89.5%; 300 DEG C of calcinations 30 minutes in retort furnace, weightless 2.8%, product is placed and within water one week, does not sink, illustrate that hydrophobic performance is fine.
Application examples
Fire retardant prepared by embodiment and comparative example is added in superpolymer polypropylene (PP), and contrast with the superpolymer polypropylene not adding fire retardant.Preparation method of sample is: it is blended that the fire retardant adopting 20 weight part above-described embodiments and comparative example to prepare respectively and 75 parts by weight of polypropylene and 5 parts by weight of maleic connect a polypropylene fusion, namely obtains polypropylene flame redardant.
Then by dry for this polypropylene flame redardant rear fender, cut into the standard batten of 130mm × 13mm × 3mm and 130mm × 6.5mm × 3mm, on CZF-3 type horizontal vertical burning determinator, carry out the test of UL-94 vertical combustion by ASTMD635-77 standard; Limiting oxygen index(LOI) is tested on HC-2 type oxygen index instrument by ASTMD2863-77 standard; According to CNS, other physicalies are tested; Its evaluation result is as shown in table 1.
Table 1 polypropylene flame redardant evaluation result
As can be seen from Table 1, the polypropylene flame redardant adding fire retardant prepared by embodiment 1-3 has good flame retardant resistance, and polyacrylic flame retardant properties can be made to significantly improve, and flame retardant properties reaches UL-94V-0 level, and limiting oxygen index(LOI) can reach more than 38.5%; Its flame retardant resistance is significantly better than fire retardant prepared by interpolation comparative example 1-4.In addition, the situation of being fuming during polypropylene burning and drippage situation, and the mechanical property of material (tensile strength, flexural strength and shock strength) have also been obtained obvious improvement.
Above the better embodiment of this patent is explained in detail, but this patent is not limited to above-mentioned embodiment, in the ken that one skilled in the relevant art possesses, can also makes a variety of changes under the prerequisite not departing from this patent aim.
Claims (9)
1. the fire retardant utilizing organo-silicone rubber waste material to produce, it is characterized in that, according to the raw material of weight part be: organo-silicone rubber waste material 18-35 part, trimeric cyanamide 5-10 part, phenyl trichlorine silicon gastral cavity 5-10, silane coupling agent 1-6 part, highly basic 5-16 part, alcohol 80-110 part, deionized water 20-50 part, fire-resistant synergistic composition 4-19 part;
Described fire-resistant synergistic composition according to the component of weight part is: carbon nanotube 4-6 part, nano mesoporous molecular screen 4-6 part, nano-attapulgite 4-6 part, micron silicon nitride 1-3 part, micrometer silicon carbide silicon 1-3 part.
2. the fire retardant utilizing organo-silicone rubber waste material to produce according to claim 1, it is characterized in that, described fire-resistant synergistic composition according to the component of weight part is: carbon nanotube 4 parts, nano mesoporous molecular screen 5 parts, nano-attapulgite 5 part, micron silicon nitride 2 parts, micrometer silicon carbide silicon 2 parts.
3. the fire retardant utilizing organo-silicone rubber waste material to produce according to claim 1 and 2, is characterized in that, described silane coupling agent be in KH550 silane coupling agent, KH560 silane coupling agent and KH570 silane coupling agent any one or multiple.
4. the fire retardant utilizing organo-silicone rubber waste material to produce according to claim 1 and 2, is characterized in that, described highly basic is sodium hydroxide and/or potassium hydroxide.
5. the fire retardant utilizing organo-silicone rubber waste material to produce according to claim 1 and 2, is characterized in that, the carbonatoms of described alcohol is 2-6.
6. the fire retardant utilizing organo-silicone rubber waste material to produce according to claim 1 and 2, it is characterized in that, described nano mesoporous molecular screen be in MCM-41 mesopore molecular sieve, MCM-48 mesopore molecular sieve, SBA-15 mesopore molecular sieve and SBA-16 mesopore molecular sieve any one or multiple.
7. a preparation method for the fire retardant utilizing organo-silicone rubber waste material to produce as described in as arbitrary in claim 1-6, it is characterized in that, concrete steps are:
(1) first organo-silicone rubber waste powder is broken into the particle that particle diameter is not more than 2mm, then adds reactor with silane coupling agent, highly basic together with unit alcohol, under stirring, microwave heating, to 30-90 DEG C, is incubated 1-3 hour; The power of described microwave heating is 0.8-1.2kW, and frequency is 1200-3600MHz;
(2) add deionized water extraction after filtering, standing separation, takes off layer liquid and is placed in reactor;
(3) in reactor, trimeric cyanamide, phenyl trichlorine silicon gastral cavity and fire-resistant synergistic composition is added again, under stirring, supersound process 0.5-1.5 hour; The power of described ultrasonication is 150-250W, and frequency is 20-40kHz;
(4) cool, filter, washing reaction product, after drying, namely obtains the fire retardant utilizing organo-silicone rubber waste material to produce.
8. the preparation method of the fire retardant utilizing organo-silicone rubber waste material to produce according to claim 7, is characterized in that, in step (1), microwave heating is to 40-60 DEG C, insulation 1.5-2.5 hour; The power of described microwave heating is 0.9-1.1kW, and frequency is 2000-2800MHz.
9. the preparation method of the fire retardant utilizing organo-silicone rubber waste material to produce according to claim 8, is characterized in that, supersound process 0.8-1.2 hour in step (3); The power of described ultrasonication is 180-220W, and frequency is 25-35kHz.
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Application publication date: 20160106 |